A kind of preparation method of perfluoroalkane
A technology for perfluoroalkane and octane is applied in the field of preparation of perfluoroalkane, which can solve the problems of difficulty in controlling the temperature of a reactor uniformly, being unsuitable for mass production, and not being able to be continuously carried out, and achieving easy control of reaction conditions and yield. High, productivity-enhancing effect
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Embodiment 1
[0031] A monel alloy reactor with an inner diameter of 80 mm and a length of 1000 mm is filled with spherical alumina with a diameter of Φ3 mm. The reactor is heated to 300°C, and a 50% fluorine-50% nitrogen mixture gas is introduced for fluorination, so that the alumina is completely converted into aluminum fluoride. Then keep the temperature of the reactor at 200°C, continuously feed 20% fluorine-nitrogen mixed gas and 10% octane-nitrogen mixed gas at the molar ratio of fluorine to octane 20:1 for reaction, and control the residence time for 5 seconds. After 10 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution until the pH value is neutral, let it stand, after layering, take the organic phase and wash it with deionized water three times, separate the organic phase and dry it with anhydrous sodium sulfate After rectification and separation, the fraction with a boiling point of 100-105°C was taken to obtain 1000 grams of perfluorooc...
Embodiment 2
[0033] Use the same equipment as in Example 1. The temperature of the reactor is maintained at 260°C, and 20% fluorine-nitrogen mixed gas and 20% octane-nitrogen mixed gas are continuously fed into the reaction according to the ratio of fluorine gas to octane molar ratio of 20:1, and the residence time is controlled for 10 seconds. After 10 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution until the pH value is neutral, let it stand, after layering, take the organic phase and wash it with deionized water three times, separate the organic phase and dry it with anhydrous sodium sulfate Afterwards, rectification and separation were carried out, and the fraction with a boiling point of 100-105°C was taken to obtain 1500 grams of perfluorooctane with a purity of 98.5% and a yield of about 75%.
Embodiment 3
[0035] Use the same equipment as in Example 1. The temperature of the reactor is maintained at 280°C, and 20% fluorine-nitrogen mixed gas and 15% octane-nitrogen mixed gas are continuously fed into the reaction according to the molar ratio of fluorine gas to octane of 25:1, and the residence time is controlled for 10 seconds. After 10 hours, neutralize the collected reaction product with 20% potassium hydroxide aqueous solution until the pH value is neutral, let it stand, after layering, take the organic phase and wash it with deionized water three times, separate the organic phase and dry it with anhydrous sodium sulfate Afterwards, rectification and separation were carried out, and the fraction with a boiling point of 100-105°C was taken to obtain 1600 grams of perfluorooctane with a purity of 98% and a yield of about 65%.
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